Method of preparing taste-modifying composition

ABSTRACT

A PROCESS FOR OBTAINING A DRY POWDERED CONCENTRATE CONTAINING THE TASTE MODIFYING PRINCIPLE FROM SYNSEPALUM DULCIFICUM DANIELL, IN A STABLE FORM WHICH US USEFUL IN COMJUNCTION WITH FOODS SUCH AS CONFECTIPNS, DESSERTS, JELLIES, JAMS, CANNED FRUIT, BEVERAGES AND COATINGS TO RENDER SOURTASTING FOODS SWEET TASTING, AND TO IMPROVE THE FLAVORR OF CERTAIN FOODS, WHILE MAINTAINING THIS TASTE MODIFYING R OF CHA ACTERISTIC FOR LONG PERIODS UNDER NORMAL ATMOSPHERIC CONDITIONS. THE CONCENTRATE IS OBTAINED BY COMMINUTING THE RIPE FRUIT OF SYNSEPALUM DULCIFICUM DANIELL, SPRAY DRYING THE COMMINUTED SLURRY OT REDUCE THE MOISTURE CONTENT BETWEN 0.5 TO ABOUT 5% BY WEIGHT, AND SEPARATING THE SPRAY DRIED POWDER OBTAINED ON A DENSITY BASIS TO RECOVER A HIGH DENSITY FRACTION. CABOHYDRATES, FATS AND PIGMENTS CAN BE REMOVED FROM THE STABLE TASTE-MODIFYING PRINCIPLE BY SOLVENT EXTRACTION TO OBTAIN CONCENTRATED COMPOSITIONS OF THE STABLE TASTE-MODIFYING PRINCIPLE WHICH ARE EMPLOYED TO FORM UNIT DOSAGE FORMS THEREOF.

United States Patent O 3,824,323 METHOD OF PREPARING TASTE-MODIFYING`COMPOSTION Robert Joseph Harvey and John Richard Fennell, Sud- Illllry,Mass., assignors to Mirlin Corporation, Hudson,

ass.

Continuation-impart of application Ser. No. 28,981, Apr. 15, 1970, nowPatent No. 3,676,149, dated July 11, 1972, and a continuation-in-part ofabandoned application Ser. No. 130,481, Apr. 1, 1971. This applicationJuly 10, 1972, Ser. No. 269,972

Int. Cl. A23l1/26 U.S. Cl. 426-429 25 Claims ABSTRACT F THE DISCLOSURE Aprocess for obtaining a dry powdered concentrate containing the tastemodifying principle from Synsepalum dulcifcum Daniell, in a stable formwhich is useful in conjunction with foods such as confections, desserts,jellies, jams, canned fruit, beverages, and coatings to rendersourtasting foods sweet tasting, and to improve the flavor of certainfoods while maintaining this taste modifying characteristic for longperiods under normal atmospheric conditions. The concentrate is obtainedby comminuting the ripe fruit of Synsepalum dulcz'fcum Daniell, spraydrying the comminuted slurry to reduce the moisture content between 0.5to about 5% by weight, and separating the spray dried powder obtained ona density basis to recover a high density fraction. Carbohydrates, fatsand pigments can be removed from the stable taste-modifying principle bysolvent extraction to obtain concentrated compositions of the stabletaste-modifying principle which are employed to form unit dosage formsthereof.

This application is a continuation-in-part of our application Ser. No.28,981, filed Apr. 5, 1970, now U.S. Pat. No. 3,676,149, issued July 11,1972, entitled Taste Modifying Composition and Method of Preparation andour application Ser. No. 130,481, filed Apr. 1, 1971, entitled UnitDosage With Variable Temporal Characteristics for Modifying Sour Taste,now abandoned.

This invention relates to a stable taste-modifying composition and toits method of preparation.

Synsepahmz dulcifcum Danieli, Sapotaceae is a plant indigeneous towest-central Africa which bears a red ellipsoid fruit commonly known asmiracle fruit. The fruit has a palatable pulp and skin and contains alarge seed. It is characterized by a pleasant taste and by the uniqueproperty, well-recognized `for over 200 years, of modifying the sweetand sour tastes in the unusual manner. It has been found that theproteineous component in the fruit binds at sites on the tongue and inthe oral cavity and, once bound at these sites, alters the way in whichthe taste receptors respond to certain foodstuffs eaten subsequently.This is particularly true of sour or acidic foods such as fruit. Anynormally sour food eaten within a short period after rst contacting thetongue with the pulp of fresh miracle fruit, causes the normally sourfood to taste pleasantsly sweet. By exposing the taste receptors on thetongue to mirable fruit, any sour tasting food can be made to tastesweet without the addition of sugar or artificial sweeteners. Forexample, fresh lemon can be made to taste pleasantly sweet by `firsteating a miracle fruit berry. It not only sweetens the lemon but alsomproves its flavor. Therefore, the fruit of Synrepalum dulcicum is ataste modifier which both sweetens and improves the flavor of normallysour tasting foods. It also selectively enhances the flavor of a fewfoods not normally regarded as tasting sour, such as mushrooms,cantalope melons, and several vegetables.

Patented July 16, 1974 ICC Two investigators have identied a specificform of the active principle in miracle fruit as a glycoprotein having amolecular weight of about 44,000. Several approaches have been exploredin attempts to isolate the active component in the miracle fruit forsubsequent use as a taste-modifying material. These attempts have metwith only very limited success either because of the form of the productobtained by these methods is less effective than the natural fruit, orit was found to be unstable at normal room temperatures under normalatmospheric conditions. This instability necessitated either very quickuse after isolation or storage at very low temperatures, either or bothof which seriously limits the utility of this material.

The prior art has regarded the active taste-modifying principle as avery labile material, accounting for the observed instability ofconcentrates maintained at normal room temperature. While some degree ofsuccess has been attained in improving stability of the active principlein the order of about a week or so, it has been found that its stabilitycould not be maintained in a powder form at normal room ambientconditions. Alternatively, the material was dissolved in specificsolvents maintained at a specic pH. These solutions had to berefrigerated to be preserved, and even then this material was not stablefor more than two weeks. Also material isolated in the past has not beeneffective as the natural fruit, particularly in its ability to improvethe ilavor of certain foods.

The active principle is present in the pulp and on the inner surface ofthe skin of the miracle fruit berry, and in its natural environment itis quickly deactivated especially when exposed to air once the skin isbroken at room temperatures. Furthermore, after the fruit has beenpicked, even prior to breaking the skin, the active material begins todegrade but at a slower rate than when the skin is broken. While theprocess by which degradation proceeds is not known exactly, it is nowbelieved that certain enzymes present in the fruit acceleratedegradation in the presence of air and moisture at normal roomtemperatures. It has been found that when the pulp of miracle fruit isfrozen and subsequently lyophilized to form a granular or powdermaterial, the product had to be either stored in a desiccator orrefrozen in order to maintain the activity of the material thatremained.

The prior art processes for isolating the active principle based uponextraction techniques not only resulted in products which are not stableat room ambient conditions, but also products that do not exhibit thefull avor enhancing characteristics. Photomicrographs of stainedsections of the fruit pulp of the berry, show that the active principleis an integral part of the cellular membranes that permeate throughoutthe fruit pulp. The glycoprotein is particularly concentrated in themembranes just beneath the skin of the berry and in the membranessurrounding the large single central seed. In order to extract theglycoprotein in a pure form, the prior art used various means forbreaking the bonds holding the glycoprotein at sites in these membranes.It is believed that the conditions employed in the extraction processesmodify the active principle so as to remove certain prosthetic groups orsugar moieties from the basic molecule, thus accounting for some of theloss of flavor-enhancing characteristics in the product obtained. Inaddition, it is believed that the removal of these groups from themolecule, alters the molecule in such a way as to eifect the physicalcharacteristics of the active substance. For instance, the materialknown as miraculin, prepared by the methods described by Kurihara &Beidler, Science, Volume 1, pages 1241-1243, 1968, both tendl toagglomerate, even when prepared as a dry powder. This relatively pureglycoprotein with a molecular weight of approximately 44,000, is notstable at room temperature and normal ambient conditions for more than aweek or two. Although the exact mechanisms are not completelyunderstood, it is believed that the bonds originally binding themolecule to the cellular membranes, as well as the sites originallyoccupied by sugar moieties, are involved in this alteration in thephysical properties of the material. Possibily degradation ordenaturation is by autolysis which degrades the taste-modifyingprinciple and causes it to lose its ability to modify the sweet and sourtastes and its ability to enhance flavors.

In applicants prior above-identified application Ser. No. 28,981, thereis described a composition containing the active principle `which isstable at room ambient conditions for two years or more in that itretains the characteristics of modifying the sweet and sour tastereceptors of the tongue and enhancing the flavor of foods. The processdescribed in the prior application for obtaining the concentrateinvolved comminuting the miracle fruit pulp and skin at low temperature,separating the vaporous and liquid components from the solid componentsat low temperature such as by freeze-drying, to form a solid residue;and finally separating the concentrate on the basis of density from thesolid residue. It was believed that a significant loss of activity wouldoccur if the comminution and separation of liquid and vaporouscomponents were not conducted at low temperatures. Accordingly, in thepreferred process, frozen carbon dioxide or water was added to thefrunit during comminution, and freeze-drying was employed to separatethe liquid and vaporous components. lIn addition, it was believeddesirable to remove as much of the water as possible from the solidmaterial rich in the active principle to minimize or eliminatedegradation of the active principle.

Applicants now have discovered that it is not necessary to comminute themiracle fruit pulp and skin at such low temperatures prior to dryingsince the time necessary to complete comminution is short and the lossof the active principle is not significant. In addition, applicants nowhave discovered that the temperature of about 40 C. or below need not beemployed during dehydration to prevent degradation of the activeprinciple since the comminuted miracle fruit can be dehydrated quicklyat slightly elevated temperatures without significant loss of the activeprinciple.

The material rich in the active principle obtained by the process ofthis invention is a powdered or granulated composition which is stablein a powdered form at normal atmospheric conditions over extendedperiods of time of a year or more and having the characteristics ofsuppressing sour taste while accentuating sweet and salt taste, andenhancing the -avor of foods ingested subsequently. The product is astable, cream-colored powder comprising the active principle admixedwith material inert with respect to the characteristic of suppressingsour taste, but excluding components that degrade the active principlepresent in the pulp and skin of miracle fruit including the activeenzymes that normally would degrade the active principle. Since theproduct of this invention is extremely stable, it can be used in manyapplications for which the unstable prior art products are not suitable.Thus, the product of this invention can be coated on or admixed withmany foods to modify their taste without the necessity of specialpackaging or quick use. The unstable prior art products are not usefulin most of these applications due to their instability believed to becaused by the hygroscopic nature of the carbohydrate components in thefruit which causes the absorbed moisture to actuate the enzymes retainedin the pulp even after dehydration.

In accordance with the process of this invention, a stable compositioncontaining the active principle in concentrated form is obtained bycomminuting depitted ripe miracle fruit containing the active principleand then separating the vaporous and liquid components. The activeenzymatic components of the ripe fruit that normally degrade the activeprinciple, are either separated from, or deactivated, in the finalconcentrate. The liquid and vaporous components are separated byspray-drying and the enzymatic components are separated by means thateffects separation on the basis of density. The processes describedtherein are based upon the approach of removing from the fruit, orotherwise deactivating, those constituents in the fruit which areresponsible for its instability or other undesirable characteristicsrather than trying to remove the active principle from its natural sitein the fruit, as have all the previous investigations. In this maner, itis believed that the active principle remains bound to the cellularfragments thus retaining its molecular structure as is the case in thenatural fruit, but in the absence of active enzymes present in thenatural fruit.

To minimize loss of the active principle after picking, the whole fruitcan be frozen to very low temperatures to await processing of the fruitpulp and skin can be proccessed immediately or within about 10 hoursafter picking to obtain the active principle concentrate. Communition ofthe fruit serves to fracture the cell walls and thereby exposesubstantially all of the active principle and facilitate subsequentprocessing. Comminution is effected to obtain particles having anaverage size of about 50 to 300 microns. The comminuted particles thenare dried by spray-drying to dry the particles. The particle temperatureduring spray-drying is controlled by controlling particle residence timein the drying gas, and temperature of the drying gas. When employing adrying gas containing a relatively large concentration of free oxygen,particle temperature is maintained below about C., preferably betweenabout 50 and 70 C. since it has been found that at elevated temperaturesthe free oxygen oxidizes a portion of the active principle therebyreducing its effectiveness for modifying the taste receptors of thetongue. In contrast, when the drying gas contains little free oxygen,i.e. less than about l0 vol. percent, or no free oxygen., slightlyhigher particle temperatures can be effected since the active principlewill not become oxidized but not such high particle temperatures as tothermally denature the proteinaceous active principle. For example, whenemploying a gas such as carbon dioxide or nitrogen containing little orno free oxygen, particle temperatures in the order of about 165 C. canbe employed for residence times normally encountered in spraydryingapparatus, i.e. in the order of a few seconds or less. When employingair, economic advantages are obtained because of the ready gas supplyand it is believed that at the particle temperatures set forth above forair, that at least a portion of the enzymes that degrade the activeprinciple become deacivated, possibly by oxidation. If the spray-driedactive principle is not separated from the material containing theactive enzyme, the product remains unstable and will be degraded quicklyat normal room condition so that it loses its taste-modifying effects.The material rich in the active principle has a substantially higherdensity than the material containing the enzyme. Therefore, theseparation of the active principle, that may contain some cellulosicmaterial, from material containing the enzyme is effected by processesthat separate materials on a density basis.

The invention will be more fully described with reference to theaccompanying figure.

Referring to the gure, washed depitted ripe miracle fruit berries aredirected through conduit 1 to comminuter 2 wherein the skin and fruitpulp are blended to an average particle size less of about 50 to 300microns. The comminuted berries then are directed through conduit 3 tolter 4 wherein the particles having an average size less than micronsare spearated from larger size particles. The larger size particles arerecycled to the comminuter through conduit 5 while the small sizeparticles in slurry form pass into hopper 7. The particles are thenwashed several times in a solvent which dissolves carbohydrates such asa mixture of ethanol (75%) and water (25%) which solvent can also removevarious pigments, some fat, and other more soluble components. Removalof these components increases the concentration of the active principle.The essentially colorless, tasteless concentrate which is very nearlynon-hygroscopic, does not result in rancidity due to oxidation of thefat components. The solid residue is pumped to spray drier throughconduit 11 by pump 8 wherein they are contacted within a dry gas such asair, carbon dioxide or nitrogen, which enters through conduit 12a. Thefruit is spray dried in chamber 12 under conditions so that the particletemperature is carefully controlled to prevent excessive oxidization orheat degradation of the taste-modifying principle as described above. Acold gas is introduced through conduit 15 into plenum 16 and throughconduits 17 so as to reduce the temperature in the spray dryer 10. Thedry particles then are directed through conduit 19 to cyclone 20 whereinthe particles are separated from the gas. The particles then aredirected through conduit 21, wherein they are contacted with air whichis pressurized by means of primary blower 22. The pressurized aircarries the particles into a separator wherein the particles areseparated on the basis of density.

The particles are introduced into the separator 25 tangentially alongthe `Walls thereof so that the particle mixture passes downwardlythrough separator 25 in a spiral path. At a vertically intermediateheight of separator 25, a secondary air stream is introduced into plenum26 which then is passed through permeable wall 27 which extends aroundthe circumference of separator 25. When the downwardly moving particlescontact the secondary air stream which is introduced radially, the lowerdensity particles are accelerated towards the center of the separator 25and are confined and segregated from the higher density particles bymeans of hopper 28. The higher density particles bypass hopper 28 andare collected in collecting means 29. The lower density particles aredirected to a second separator 30 and introduced tangentially therein sothat they are passed downwardly in a spiral path. A secondary gas streamis introduced into plenum 31 and through permeable wall 32 extendingaround the circumference of the separator 30. The low density particlesare collected in hopper 31a and the higher density particles arecollected in collector 32a in a manner described with reference toseparator 25. The separators 25 and 30 are more fully described in acopending application filed concurrently herewith by Robert J. Harveyand entitled, Method and Apparatus for Separating Particles on the Basisof Size of Density,

The gas obtained from cyclone 20 contains moisture and some particles.Accordingly, when air is not employed, prior to recycling the gas tospray drier 10 it is filtered in filter 35 and directed to condenser 36wherein liquids are condensed therefrom and remove through conduit 37.The gas is then further dried in the presence of a desiccator in drier37a. The dried gas is then directed to plenum 11 by means of primaryblower 38. The gas is heated in heater 40 to a temperature of about 175to 200 C. to accelerate-liquid evaporation in the spray drier 10. Makeupdry gas is introduced from reservoir 41 into the primary blower 38. Whenair is used as the drying gas, the system is operated as an open cyclesystem with the incoming air entering the system at filter 35 beingexhausted to theatmosphere directly from the cyclone separator 20.

The preferred process of this invention is based upon the discovery thatdegradation of the active principle in the fruit is initiatedimmediately after the ripe fruit is picked, and that degradation of theactive principle in its natural environment is accelerated by increasedtemperature and by contact with air. Thus, it is preferred to processthe ripe miracle fruit quickly, and at a relatively low temperature inorder to obtain a high yield of the active principle. Preferably, thepicked fruit is washed in water and then depitted at about l to 4 C. Thefruit can be stored in a frozen state to await processing or can beprocessed immediately to obtain the active principle. When stored,temperatures of about 40 C. or less are employed to arrest degradation.Since it is difiicult to remove the pit or seed from the frozen berry,it is preferred to depit the berry prior to frozen storage. The depittcdberry, regardless of whether it has been stored previously or whether itis processed directly after having been picked, is comminuted to obtainparticles having an average size less than about microns, preferablyless than about 50 microns. Comminution can be effected at normal roomambient conditions and generally is completed within a few seconds.Comminution can be eiiected by blending, grinding or milling. Thepreferred method is by use of a Fitz-mill.

During spray drying, the particles are contacted with a dry gas streamsuch as air, carbon dioxide or nitrogen at an elevated temperature. Thedried particles contain from about 5 wt. percent water down to theamount of water comprising water of hydration in the protein molecule orabout 0.5 wt. percent.

The powdered product then is further separated on the basis of density.The separation of the material containing the concentrated activeprinciple from the other dry material is based upon the fact that thematerial rich in the active principle is more dense than the othermaterial. Thus, the mixture of inerts and active material describedabove can be separated by any convenient density separation methodincluding settling from a suspension of the mixture in liquid, the useof fiuidizing bed technique, or through the use of cyclone typecentrifuge.

The solvent extraction step to remove carbohydrates is conducted byadmixing the comminuted ripe fruit with the solvent one or more timesand then separating the remaining solid from liquid, as for example byltration and then removing residual solvent by evaporation. The solventextraction to remove carbohydrates can be conducted either prior to orsubsequent to the spray-drying step. The solvent employed dissolves thecarbohydrate without dissolving or degrading a substantial portion ofthe active principle. Representative suitable solvents include water,and ethanol-water mixtures or the like. When employing water or solventscontaining water, prior to the spray-drying step, the solvent extractionstep should be conducted relatively qiuckly, i.e. for less than about l0or l5 minutes since water tends to accelerate degradation of the activeprinciple by the enzymes in the fruit. It is preferred to condut thesolvent extraction step prior to spray drying since residual solvent inthe comminuted fruit can be removed therefrom in the spray-drying step.

In another aspect of the present invention, the concentrate containingthe active principle can be treated further to improve its appearancefor use in foods while not degrading the active principle. Thus, theconcentrate can be treated to remove further any reddish color of theripe fruit by introducing a bleaching agent into the comminuted pulpprior to spray drying or by additional solvent extraction using analcohol-Water mixture. A suitable bleaching agent is sodium suliite..Furthermore, it has been found that miracle fruit contains certain fattymaterials which upon oxidation may impart a slightly rancid taste to thestable product. Accordingly, the spray dried product can be treatedeither after the spray-drying step or the density separation step with asolvent extraction step using a solvent for fats which. is subsequentlyseparated from the end product using conventional filtering techniques.Suitable solvents include acetone or ether. The last trace of thesolvent is removed. from the concentrate containing the active principleby evaporation which is readily accomplished with such volatilesolvents.

In one aspect, the present invention provides a stable compositioncontaining a higher concentration of the tastemodifying principle thanis obtained by the process disclosed in the above-identified copendingapplication Ser. No. 28,981. It has been found that up to about 65weight percent of the product obtained by our prior process comprisecarbohydrates and other soluble components which can be removed from thecomposition by solvent extraction. The stable taste-modifying principlein the composition of this invention and that disclosed in priorapplications are the same since the carbohydrates are inert with respectto the taste-modifying characteristics of these compositions. However,the concentrated composition of this invention provides a substantialadvantage over that disclosed by our prior application since muchsmaller unit dosage forms can be prepared therefrom. As disclosed by ourprior application Ser. No. 130,481, unit dosage forms contain from about20 to 100 milligrams of the prior stable taste-modifying material. Incontrast, the low carbohydrate compositions of the invention are usefulin unit dosage forms in amounts from about 1 to 25 milligrams.

The composition of this invention comprises particulate solid rich inthe taste modifying principle of Synsepalu'm dulcijcum Daniell forsuppressing sour taste and enhancing sweet and salt taste obtained fromthe ripe fruit of Synsepalum dulcfcum Daniell which is substantiallyfree of the components of the ripe fruit that degrade the tastemodifyingprinciple and substantially free of the hygroscopic soluble carbohydrateof the ripe fruit. The tastemodifying composition contains less thanabout 25 weight percent carbohydrates, as compared to about 70 weightpercent in the product obtained by the process of Ser. No. 28,981.

The stable taste-modifying composition substantially free ofcarbohydrates can be employed to form unit dosage forms that areeffective for varying the time period the composition modifies the tastereceptors of the tongue.

In designing a unit dosage form, there are a number of variables to beconsidered, the most important of which are:

(1) The level of activity of the taste modifying effect (level ofsweetness and the qualitative taste characteristics of the fiavorenhancing effect);

(2) The duration of the taste-modifying effect;

(3) The speed of reaction; that is, the time after chewing the unit doseform before it becomes fully effective;

(4) The economics of the separate unit dose form.

All of these above variables are affected by both the dose, or theamount, of the taste-modifying composition, as well as the particle-sizedistribution of the active principle.

The smaller the particle size, of the active principle, the more rapidlythe full taste-modifying effect becomes effective. Therefore, thisrelationship is relatively straight-forward. Similarly with theeconomics, the lower the dose, the more favorable the economics,particularly for higher volume production.

The relationship of the level of sweetness and quality of theflavor-modifying characteristics, and the duration or thetaste-modifying effect, as a function of the particle size distribution,are all much more involved. As one holds the particle size distributionconstant, and increases the dose, one finds that there are two distinctpatterns of response. From a unit dose less than 1 mg. to a dose up toabout to 20 mg., there is a rapid increase in the level of sweetnessthat one perceives from otherwise sour foods eaten subsequently toadministering the separate unit dose form. Above about mg., increasingthe dose further, does not cause a further increase in the level ofsweetness. In other words, the saturation point has been reached.

Similarly with the duration of the taste-modifying effect. As the doseis increased from less than 1 mg. to about mg., one notes that theduration of the taste-modifying effect is extended from a few minutes tomore than an hour. As the dose is increased much above a dose of 25 mg.,there is not much further increase in the duration of thetaste-modifying effect. On a cost effectiveness basis, there is noadvantage in having a dose greater than 25 mg.

If one holds the dose constant, say at 10 to 15 mg., and varies theparticle size of the active ingredient, one also notes changes in boththe level of taste-modifying activity as well as the duration of theeffect. However, the upper and lower limits of particle size aredetermined by other considerations. On the large particle size, one ndsit difficult to formulate mixtures of dry powders when the particle sizeis larger than about 300g. Similarly, when the particle size drops muchbelow 50u, certainly below 10g, one finds it difficult to workeffectively with such fine material. Therefore, the range of particlesize of interest is 10 to 30C/.L This particle size range for a fixeddose of about 12 mg., gives a duration of response from a few minutes toabout one hour. Of course, if one wants a fast-acting response, oneshould include a significant fraction of the active material with aparticle size of less than 50,11..

The unit dosage form can be of any physical form, most usually a powderor a tablet. Active principle of varying particle size is formed by anyconventional comminuting process, for example, ball-milling, pestal andmortar or other dry brinding processes such as Fite milling. The activeprinciple is comminuted and then screened to isolate various particlesize ranges.

The following examples illustrate the present invention and are notintended to limit the same.

EXAMPLE I Ripe miracle fruit berries are picked and washed in coldwater.

The fruit then is depitted in a juicer comprising a perforatedcylindrical housing with a rotating brush extending along thecylindrical length, the ends of which contact the inside cylinder wall.During rotation, the berries tumble and are pressed against theperforated housing causing the juice and pulp material to pass throughthe holes, leaving the pits in the cylinder. The juice and pulp arepumped to a mill to comminute the particles. The particles are screenedto pass particles having an average size less than 150 microns (100mesh) while the particles larger than 150 microns are recycled to thegrinding step. Cooling is desirable during grinding to prevent thermaldegradation.

The particles are then washed twice in a cold solvent containing 75%ethanol and 25% distilled water. The solid material is separated fromthe liquid phase.

The slurry (solid phase) is then pumped to a spray drier wherein theparticles contact an incoming stream of dry air, at a temperature suchthat the particle temperature does not exceed more than about C.,usually from about 60 C. to about 70 C. The average contact time of theparticles and gas in the spray drier particles is less than about asecond. The moisture content of the final spray dried powder is about 3to 5 wt. percent.

The fine dried powder obtained from the spray drier is introduced into apneumatic cyclone-type separator, whereby the material rich in theactive principle is concentrated near the inside wall and the othermaterial is concentrated closer to the center of the cyclone. Themixture to be separated is introduced into the top of the cyclone andcaused to move in a circular path down the inside wall. The product isseparated from the lower density material by a baffle located at theinterface between the high and low density material. The lower densitymaterial is recycled until substantially all the active principle isseparated. The concentrated product can be recycled if necessary, toachieve any degree of separation from the lower density material.

The powder obtained by this process has a moisture content of l-3 wt.percent; it is room temperature stable even when stored in the openatmosphere for at least a year or more; and it can be used to produceunit dose forms including tablets or aerosol sprays. The dry powderobtained contains about 40% protein, about 25% carbohydrates, about 3%moisture, and the remainder fat and inerts.

The procedure of Example I was followed with the additional step ofwashing the comminuted particles with acetone to solubilize selectivelythe fats remaining in the spray-dried powder.

The slurry then is evaporated in air'at an ambient temperature to removethe residual acetone and to reduce the moisture content of the powderfrom about 3 wt. percent to about 1 wt. percent or less. It is notnecessary to employ a controlled atmosphere in the acetone-removal step.After the acetone is removed, the powdered product is directed to thepowder separation steps as described in Example I.

' EXAMPLE III The procedure of Examples I and II was followed with anadditional step of adding sufficient sodium sulfite during the blendingstep so that the amount of sodium sulfte added represents 1% of the dryweight of the final product. The sodium sulfite was added to bleach thenormally red or pink pulp and skin so that the Ifinal powdered productobtained is white.. The sodium sulfite also functions as an antisepticagent for micro-organisms.

EXAMPLE IV This example illustrates a typical active principleformulation, a method for preparing chewable tablets therefrom and theresults of tests on subjects after having chewed the tablets containingthe powdered product produced according to Example I, above.

The formulation used to make the tablets is set forth in Table I.

The following procedure was carried out at a temperature of 68-75 F.with relative humidity or less than 50% to prepare the tablets. Theingredients set forth in Table I were mixed and blended, including theactive principle obtained by the process of Example I at a concentrationof 20 milligrams active principle per tablet. The particle size rangedfrom less than 50p. to 150g.

The tablets were made by pressing the formulation in a Stokes RotaryTablet Press (B2) using a standard 12/32 inch concave punch. The tabletshad a hardness (Monsanto) of 3.0-3.5 kg. and weighed 400 milligrams.

The tablets were tested for their taste-modifying effects by a procedurethat determines the apparent sweetness effected by a standard citricacid solution after chewing the tablet containing the active principle,and comparing this sweetness to sugar solutions of known concentration.Each subject rinsed his mouth for one minute with distilled water. Thetablet containing the active principle then was thoroughly chewed forone minute. Then the subject rinsed his mouth with distilled water forthirty seconds and waited two minutes. The subject then tasted astandard citric acid solution (.03 M). After tasting the citric acidsolution, the subject rinsed with distilled water for thirty seconds.After experiencing the sweetness of the citric acid solution, thesubject was then required to compare the sweetness experienced withstandard sugar solutions of known concentrations to determine therelative sweetness of the citric acid solution. The results for eachformulation as a function of time was as shown in Table II.

The period of effectiveness is affected by the extent of salivation; themore one salivates the faster the effect wears off. The above data wascollected by stimulating at frequent intervals. It is not likely thatthe period of effectiveness could be reduced by more than 10% or 15% byincreased salivation caused by the intense taste testing. However, ifone administers the active principle, but then does not eat or otherwisestimulate the taste receptors or does not otherwise cause increasedsalivation, then the period of effectiveness stated in Table II could beextended as much as 50% TABLE 11.-ORGANOLEPTIC EVALUATION Formulation:Table I Tast-modifying effect became effective Instantly (less than l0seconds). Retained full level of sweetness 45 minutes. Time after whichit became 0bjectionable minutes. Time before the effect was completelygone minutes.

What is claimed is:

1. In a process for obtaining a composition for suppressing sour tasteand enhancing sweet and salt taste, which retains its taste-modifyingcharacteristics at normal room temperature for long periods, saidcomposition comprising particulate solid material rich in thetastemodifying principle of Synsepalum dulcz'fcum Daniell forsuppressing sour taste and enhancing sweet and salt taste obtained fromthe ripe fruit of Synsepalum dulcfcum Danieli, which solid issubstantially free of the active components of the ripe fruit thatotherwise degrade the taste-modifying principle; which process comprisescornminuting the ripe fruit to rupture the cellular structure thereof,drying a portion of the comminuted ripe fruit including thetaste-modifying principle and dissociating the enzymatic components ofthe ripe fruit that degrade the taste-modifying principle from thematerial rich in the taste-modifying principle of the comminuted ripefruit, that improvement wherein:

the portion including the taste-modifying principle is heated to atemperature up to about C. during said drying without oxidizing asubstantial portion of the taste-modifying principle.

2. The process of claim 1 wherein pigments in the ripe fruit are removedfrom the portion including the taste-modifying principle by solventextraction.

3. The process of claim 1 wherein fats in the ripe fruit are removedfrom the portion including the taste-modifying principle by solventextraction.

4. The process of claim 3 wherein pigments in the ripe fruit are removedfrom the portion including the taste-modifying principle by solventextraction.

5. The process of claim 1 wherein the soluble carbohydrates are removedfrom the portion including the taste-modifying principle by solventextraction.

6. The process of claim 5 wherein pigments in the ripe fruit are removedfrom the portion including the tastemodifying principle by solventextraction.

7. The process 0f claim 5 wherein fats in the ripe fruit are removedfrom the portion including the taste-modifying principle by solventextraction.

8. The process of claim 7 wherein pigments in the 'ripe fruit areremoved from the comminuted ripe fruit by solvent extraction.

9. The process of claim 1 wherein the portion including thetaste-modifying principle is spray dried by heating in a gas.

10. The process of claim 9 wherein the portion including thetaste-modifying principle is spray dried in heated air to raise thetemperature of the portion including the taste-modifying principle toabout 60 C. to 80 C.

11. The process of claim 10 wherein pigments in the ripe fruit areremoved from the portion including the taste-modifying principle bysolvent: extraction.

12. The process of claim 10 wherein fats in the ripe fruit are removedfrom the portion including the tastemodifying principle by solventextraction.

13. The process of claim 12 wherein pigments in the ripe fruit areremoved from the comminuted ripe fruit by solvent extraction.

14. The process of claim 10 wherein the soluble carbohydrates areremoved from the portion including the taste-modifying principle bysolvent extraction.

15. The process of claim 14 wherein pigments in the ripe fruit areremoved from the portion including the taste-modifying principle bysolvent extraction.

16. The process of claim 14 wherein fats in the ripe fruit are removedfrom the portion including the tasternodifying principle by solventextraction.

17. The process of claim 16 wherein pigments in the ripe fruit areremoved from the comminuted ripe fruit by solvent extraction.

18. The process of claim 9 wherein the comminuted ripe fruit is driedprior to said dissociating.

, 19. The process of claim 18 wherein the comminuted ripe fruit is spraydried in heated air to raise the temperature of the comminuted ripefruit to about 60 C. to 80 C.

20. The process of claim 19 wherein fats in the ripe fruit are removedfrom the comminuted ripe fruit by solvent extraction.

21. The process of claim 19 wherein pigments in the ripe fruit areremoved from the comminuted ripe fruit by solvent extraction.

22. The process of claim 19 wherein the solublecarbohydrates are removedfrom the comminuted ripe fruit by solvent extraction.

23. The process of claim 22 wherein pigments in the ripe fruit areremoved from the comminuted ripe fruit by solvent extraction. v

24. The process of claim 22 wherein fats in the ripe fruit are removedfrom the comminuted ripe fruit by solvent extraction.

25. The process of claim 24 wherein pigments in the ripe fruit areremoved from the comminuted ripe fruit by solvent extraction.

, References Cited UNITED STATES PATENTS 3,676,149 7/1972 Fennell et al.99-140 R MORRIS O. WOLK, Primary Examiner S. MARANTZ, Assistant ExaminerU.S. C1. X.R.

